基于多指标评价法的蒲公英提取工艺优化

以超声提取法提取蒲公英有效成分，选择总黄酮、咖啡酸、绿原酸和菊苣酸为评价指标，结合AHP-CRITIC法计算各指标权重；在单因素试验的基础上，利用Box-Behnken法优化蒲公英超声提取工艺。实验结果表明超声提取法提取蒲公英的最优提取工艺参数为：液料比5∶1,甲醇浓度60%,提取时间26 min,在此工艺条件下预测综合评分为73.26,验证实验所得综合评分为74.13±2.63,RSD为3.55%。本研究优化的蒲公英超声提取工艺适合于蒲公英中总黄酮、咖啡酸、绿原酸和菊苣酸的提取，其工艺稳定、可靠，可为蒲公英资源的开发和利用提供参考。     

咖啡因提取的综合性实验教学

介绍了一个综合性化学实验。该实验以绿茶为原料,95%的乙醇为提取剂,通过索氏提取器提取、常压蒸馏及升华等实验操作,得到咖啡因产品。通过超高效合相色谱法（Ultra Performance Convergence Chromatography,UPC2）确定咖啡因的含量,熔点测定法及1H-NMR归属分析表征结构。本实验将经典的有机化学实验和先进的分析测试仪器相结合,提高了学生的实验综合能力,激发了学生的科研兴趣和探索精神。     

银杏根中黄酮类化合物的分离分析

采用丙酮浸泡、回流从银杏根中提取得到黄酮，以HPLC法分离测定其中的槲皮素含量。实验结果表明：银杏根黄酮存在槲皮素甙，不含山奈酚、异鼠李素等物质。     

西府海棠花中蛋白质提取及动态含量研究

采用超声波辅助提取法,优化西府海棠花朵中蛋白质的提取工艺条件,并在最佳工艺条件下研究了西府海棠花朵中蛋白质含量的动态变化。在单因素实验基础上,采用正交实验对蛋白质的主要提取工艺参数进行优化,结果为：采用pH=10的Tris-HCl提取液、液料比为70∶1（mL/g）,在30℃、400 W下超声提取120 min。在该最佳提取工艺条件下,测得开花2周的花朵中蛋白质含量最高,提取率为0.023 5;开花3周的花朵中蛋白质含量最低,提取率仅为0.004 48。说明开花2周的西府海棠花的利用价值最高。该实验可作为农林院校4~5学时的分析化学实验课的综合实验。     

提取方式对信阳山茶油品质影响与评价研究

采用超临界CO2法、超声波辅助提取法和索氏提取法提取山茶籽油,对它的理化指标、脂肪酸组成进行测定,并对茶粕有效成分进行分析。研究表明,超临界CO2法和超声波法提油率高,环保安全性和工艺效率好;索氏法提取的油茶籽油酸值过大;从茶粕有效成分含量来看,超声波辅助提取法更优。综合考虑3种提取方法,超声波辅助提取山茶油品质最优。     

鹿茸中18种性激素的提取技术研究

建立一种高效提取鹿茸中雌二醇、雌三醇和睾酮等18种性激素的方法.采用超声波提取法进行提取,液相色谱-串联质谱定性,以回收率为评价指标,分别考察提取溶剂、提取剂用量和提取时间对18种性激素提取效率的影响,并以提取效率实验对建立的方法加以验证.提取溶剂为甲醇,用量为10 m L,超声波提取时间为20 min时,利用优化的超声提取操作步骤进行提取效率实验,18种性激素回收率为73%~116%,实验结果表明在该条件下的超声波提取法快速、准确,重现性好,可同时有效提取鹿茸中的18种性激素,为鹿茸及其制品中性激素前处理提供参考方法.     

人参中总皂甙的超声波快速提取方法研究

建立了人参中总皂甙超声波半微量快速提取方法，与索氏提取法相比，此法提取时间由索氏法的1－2个工作日缩短到30min，节省大量试剂，综合提取效率提高数十倍，与索氏提取法对照分析表明，此法可完全满足人参中总皂甙的快速测定要求。     

博落回生物总碱提取方法研究

对比酸水浸提法、醇提取法、索氏提取法的提取率,探讨博落回中总生物碱的最佳提取方法。从提取率、生物碱含量、有机溶剂消耗方面对酸水浸提提、乙醇提取以及索氏提取等方法的比较得出以下结论:索氏提取法中有机溶剂的回收率是最高的,酸水浸提法次之,醇提取法对原料的利用率相对来说是最低的。     

果品总酸度的测定

以苹果为实验材料,采用水浴浸提法和超声波辅助提取法提取果酸,通过正交实验优化果酸的提取工艺,并用酸碱滴定法测定总酸度。实验结果表明：水浴浸提法的最佳提取条件为：温度80℃,时间90 min,苹果质量15 g,果酸含量为4.476 3 g/kg;超声波辅助提取法的最佳提取条件为：温度70℃,时间30 min,苹果质量15 g,果酸含量为4.791 8 g/kg。     

翻白草中鞣质的微波提取工艺研究

采用微波辅助提取方法,以提取剂浓度、pH值、液固比、微波提取时间、温度等为考察因素,并以提取物中总鞣质的提取率为评价指标,使用磷钼钨酸-干酪素分光光度法为定量测定方法,在单因素实验的基础上,通过正交实验优化翻白草中鞣质的提取工艺.实验结果表明,最佳提取条件为:使用70%甲醇作为提取剂、液固比40∶1、提取液pH为8.0、提取温度为40℃、提取时间为10 min.还对翻白草不同部位(根、茎、叶)的鞣质含量进行分析,发现根部中鞣质的含量最大,其次为茎和叶.此外,采用高效液相色谱法对翻白草中鞣质的种类进行定性分析.     

对氨基酚络合萃取机理的探讨

对氨基酚络合萃取机理的探讨;对氨基酚; 络合萃取; 萃取机理; 萃取反应热     

Focused microwave aqueous extraction of chlorophenols from solid matrices and their analysis by chromatographic techniques

Open-vessel focused microwave (FMW) extraction with a purely aqueous carbonate solution was used for the extraction of chlorophenols from various solid matrices. After SPE on C18-bonded silica, the analytes were determined as such by LC-UV or, as their acetyl derivatives, by GC-ECD. The FMW aqueous extraction is efficient and rapid and no organic solvents are used. PCP was detected in several solid samples, with recoveries of 101-115% (RSD, 2-4%) relative to Soxhlet extraction. Similar recoveries were obtained for the other chlorophenols for spiked samples.     

超声辅助液液萃取法提取烟用香精成分的研究

采用超声辅助液液萃取法(ULLE)提取某品牌烟用香精成分,GC-MS对其进行分析,研究了不同萃取剂、萃取时间和萃取温度对分析结果的影响,初步确定了最佳条件为:以二氯甲烷为萃取剂,饱和NaCl溶液作水相,室温下超声萃取5 min.又分别与同时蒸馏萃取法(SDE)和传统的液液萃取法(LLE)作以比较,对ULLE法和SDE法鉴定出的化学成分、重现性和定量值进行了对比.结果表明:超声辅助液液萃取具有操作简便、快速、节能、萃取效率高、重现性好等特点,适合于烟用香精成分的提取.     

中草药化学成分提取新技术

介绍五种提取新技术棗微波萃取技术、超临界二氧化碳萃取技术、超声波提取技术、半仿生提取技术和酶法的原理和特点,以及这些新技术近年来在中草药化学成分提取工艺中的研究应用现状,并展望了它们的应用前景。     

Improved extraction and clean-up of imidazolinone herbicides from soil solutions using different solid-phase sorbents

Extraction and quantification of herbicide residues from soil are important in understanding the behaviour of persistent herbicides. This research investigated extraction and clean-up methods for imidazolinone herbicides from soil and soil amended with organic material. A series of solvent mixes, pH conditions and sorbents was tested. Across three imidazolinone herbicides: imazapyr, imazethapyr and imazaquin, 0.5 M NaOH extraction gave greater than 90% recovery from soil samples; however, 0.5 M NaOH:MeOH (80:20) resulted in higher recovery for imazaquin, but not for the other two herbicides. Of the sorbents tested, the use of chromatographic mode sequencing using C₁₈ and SCX sorbents provided consistent high (>85%) recovery of all three herbicides from soil and separation of the herbicides from other soil components by high performance liquid chromatography (HPLC). These two methods will allow high recovery of these imidazolinone herbicides from soil and have the ability to detect these herbicides without interference from other soil components.     

Supercritical fluid extraction

Supercritical fluid extraction (SFE) provides for the first time a viable option to conventional and widely used Soxhlet extraction. The ability to change the solvating power of a single supercritical fluid by changing its density is an exceedingly attractive feature. An environmentally safe alternative such as supercritical carbon dioxide to organochlorine solvents which are widely used today in many government and industrial analytical laboratories for sample preparation is desirable. SFE may also constitute a viable alternative to other popular sample preparation techniques such as liquid-liquid extraction, solid phase extraction and purge/trap. Much research, however, must be done in order to understand, optimize and apply this technology. For example, (a) automation of extraction, (b) matrix effects, (c) new fluids/modifiers/additives, (d) trapping efficiency, (e) recovery of extracted analytes, and (f) extraction kinetics are some areas which need a greater understanding. This review is concerned with many of these topics as they relate to trace organic analysis wherein SFE is the primary sample preparation technique.     

Comparison of alternative and conventional extraction techniques for the determination of zearalenone in corn

Naturally contaminated corn samples of different origin were extracted using two conventional techniques (blending and shaking) and three alternative approaches (ultrasonic extraction, accelerated solvent extraction, and microwave-assisted extraction). Use of the same extraction mixture for all trials enabled the efficiency of the various extraction techniques to be compared. Extracts were filtered and directly analyzed by LC–ESI–MS, without further clean-up. The yield from the alternative extraction techniques showed efficiency to be higher than for conventional techniques. In particular, microwave-assisted extraction was slightly superior to other techniques.     

A Unified Sample Preparation System for Extraction of Various Analyte/Matrix Combinations

A supercritical fluid extraction/enhanced solvent extraction system (SFE/ESE) was used to remove polar and non-polar analytes from various matrices. Extraction of environmental pollutants from soil, additives from low density polyethylene, sulfa drugs from animal tissue, and drug from tablet was performed using both SFE and ESE. Results showed that a single instrumental system can be used to perform both ESE with organic solvents and SFE with carbon dioxide-based fluids. Each method has its own unique advantages and applications. The ability to carry out both solvent extraction and supercritical fluid extraction with one system has obvious economical advantages.     

Effect of Ultrasound-Assisted,Microwave-Assisted and Ultrasound-Microwave-Assisted Extraction on Pectin Extraction from Industrial Tomato Waste

This work aimed to study the effect of ultrasound-assisted (UAE), microwave-assisted (MAE), and ultrasound-microwave-assisted (UMAE) methods for pectin extraction from industrial tomato waste. The overall performance index from the fuzzy analytical method with three criteria, pectin yield, galacturonic acid, and lycopene content, was applied to evaluate the best extraction conditions by using the weight of 75, 20, and 5, respectively. The UAE conditions was performed at a temperature of 80 °C for 20 min with the variations in the extraction pH and the solid liquid (SL) ratio. The best UAE conditions with high pectin yield, and high total carboxyl group, as well as a lycopene content, was the pH of 1.5 and the SL ratio of 1:30. The MAE conditions was performed with variations in the microwave powers and times. The results showed that the best MAE conditions were 300 W for 10 min, which gave high pectin yield with high galacturonic acid and lycopene content. Various conditions of UMAE at the best conditions of MAE and UAE were performed and exhibited that the UAE had more positively affected the pectin yield. However, the FTIR spectra of obtained pectins from different extraction techniques showed a similar pectin structure.     

Comparative study of optimised BCR sequential extraction scheme and acid leaching of elements in the certified reference material NIST 2711

The optimised BCR sequential extraction procedure and a 4 h 1 mol L⁻¹ HCl partial extraction have been performed on the NIST 2711 reference material for a suite of 12 elements (Cd, Sb, Pb, Al, Cr, Mn, Fe, Co, Ni, Cu, Zn, As) using magnetic sector ICP-MS. A pseudo-total aqua regia digest of NIST 2711 has also been undertaken for quality assurance purposes, and comparison of the sum of the four BCR fractions, which included an aqua regia digest on the residue, with the pseudo-total aqua regia digest has been used to assess the accuracy of the BCR partitioning approach. As a result of this work, discrepancies between previous studies about BCR partitioning of elements in NIST 2711 have been discussed and an increase in confidence about the use of BCR partitioning scheme on seven elements (Cd, Pb, Al, Mn, Fe, Cu, Zn) in this standard material has been obtained. On the other hand, BCR partitioning for Sb, Cr, Co, Ni and As has been provided for the first time. Partial extraction results are also reported for the same 12 elements analysed by the optimised BCR procedure, with the partial extraction results exhibiting a strong correlation with the sum of the three labile steps of the BCR procedure.